HRID584674

反应详情

EQUATION

反应方程式

HRID 584674 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

4,5-Dinitro-1,2-phenylenediamine (890 mg, 4.5 mmol) (G. W. H. Cheeseman, J. Org. Soc. 1170-5, 1962) was mixed with 1-phenyl-1,2-propanedione (800 mg, 5.4 mmol) in ethanol (18 ml). The mixture was heated to reflux for 4 hours. The ethanol was removed by evaporation and the remaining brown oil was suspended in dichloromethane (20 ml). Purification by column chromatography on silica gel eluting with dichloromethane followed by recrystallisation from ethanol yielded the title compound (200 mg, 14%).

WORKUP

后处理

  1. temperatureThe mixture was heated
  2. temperatureto reflux for 4 hours
  3. customThe ethanol was removed by evaporation
  4. customPurification by column chromatography on silica gel eluting with dichloromethane
  5. customfollowed by recrystallisation from ethanol